CN102863154A - Method for preparing super-hydrophobicity surfaces - Google Patents
Method for preparing super-hydrophobicity surfaces Download PDFInfo
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Abstract
The invention discloses a method for preparing super-hydrophobicity surfaces. A silane coupling agent containing reactivity amino serves as a catalyst to prepare amino modified hollow silica nanometer microspheres; the amino modified hollow silica nanometer microspheres are reacted with epoxy group modified titanium dioxide nano particles to form nano composite particles in raspberry-shaped structures; and the nano composite particles in raspberry-shaped structures are modified through long-carbon-chain fluorine-containing substances to prepare the super-hydrophobicity surfaces. The method for preparing super-hydrophobicity surfaces is characterized in that templates are not needed in the preparing process of the amino modified hollow silica nanometer microspheres; and the chemical bonding reaction between the amino modified hollow silica nanometer microspheres and the epoxy group modified titanium dioxide nano particles is used for preparing the nano composite particles in raspberry-shaped structures. The super-hydrophobicity surfaces are hopeful for being applied to heavy metal ion absorption and separation, harmful gas absorption and decomposing and micro-carrier aspects in relevant separation processes.
Description
Technical field
The present invention relates to a kind of preparation method of super hydrophobic surface.
Background technology
Wetting property is one of critical nature of solid surface.So-called super hydrophobic surface generally refers to contact angle with water greater than 150o, and roll angle is less than the surface of 10o.One of essential condition of preparation super hydrophobic surface is to make up uneven surface.Raspberry shape structure nano composite particles be a kind of on pattern the nuclear shell structure nano composite particles of similar raspberry.Utilize the chemical covalency keyed jointing between the different functional groups to make up a kind of method that raspberry shape structure is preparation raspberry shape structure nano composite particles, because the raspberry shape structure nano composite particles of preparation is subjected to environment pH value and Solvent effect less by this method, therefore, this method is widely used.Because the singularity of pattern and composition, in the process of preparation super hydrophobic surface, raspberry shape structure nano composite particles not only can make up uneven surface, can also introduce other physics or chemical property.Therefore, utilize raspberry shape structure nano composite particles to prepare super hydrophobic surface very large researching value is arranged.
The research that utilizes hollow microsphere to prepare super hydrophobic surface had caused people's concern in recent years.At present, widely used hollow microsphere preparation method is template.At first preparation uses template as the nucleocapsid structure of nuclear, thereby the template of then removing in the nucleocapsid structure obtains hollow structure.The report for preparing hollow microsphere about this method is a lot.For example: among the CN 1631951A, at silicon dioxide nanosphere surface chemistry keyed jointing one deck polystyrene, then fall silicon dioxide nanosphere with hf etching by micro-emulsion polymerization, prepared hollow microsphere; Among the CN 101172609A, use polystyrene microsphere as template, in deionized water and ethanol medium, take ammoniacal liquor as catalyzer with etching agent, make and contain mercaptosilane coupling agents at the Surfaces of Polystyrene Microparticles hydrolytie polycondensation, formation is with the sulfydryl silica shell, and polystyrene microsphere is etched away by ammoniacal liquor simultaneously, finally forms hollow microsphere; Among the CN 1795978A, use polystyrene microsphere as template, prepared titanium dioxide/polyacrylonitrile/polystyrene Core-Shell Structures ball that declines, 600 ℃ of lower calcinings 120 minutes, prepared nano hollow microsphere of composite titania/inorganic carbon subsequently.But need preparation and the removal process of template by the template synthesis hollow microsphere, technique is loaded down with trivial details, and products therefrom does not have hydrophobic property.Therefore, exploring the simple hollow microsphere preparation method of technique, and utilize hollow microsphere to make up super hydrophobic surface, is the research with very strong theory and practice meaning.
Summary of the invention
Content of the present invention provides a kind of preparation method with super hydrophobic surface.
Preparation method of the present invention is simple, mainly may further comprise the steps:
A. prepare amido modified hollow silica Nano microsphere: will be with the silane coupling agent of reactive amino and the mixture of tetraethoxy, be added drop-wise in the deionized water, stirring reaction is 2～8 hours between 20～40 ℃, obtain amido modified hollow silica Nano microsphere, wherein said silane coupling agent with reactive amino is APTES, the 3-TSL 8330, N-β (aminoethyl)-γ-aminopropyl methyl dimethoxysilane or N-β (aminoethyl)-γ-aminopropyl triethoxysilane a kind of, being 2～5:1 with the silane coupling agent consumption of reactive amino and the mol ratio of tetraethoxy consumption, is 1:4～8 with the silane coupling agent of reactive amino and the mixture of tetraethoxy and the mass ratio of deionized water;
B. prepare epoxy group modified titanium dioxide nano-particle: deionized water is added drop-wise to sequestrant, in the mixture of ethanol and tetrabutyl titanate, stirring reaction 8～12 hours, centrifugal drying, grind afterwards and make titanium dioxide nano-particle, with prepared titanium dioxide nano-particle with join respectively in the solvent with the silane coupling agent of reactive epoxy group(ing), stirring reaction is 8～12 hours between 30～60 ℃, grind afterwards and make epoxy group modified titanium dioxide nano-particle, wherein said sequestrant is methyl aceto acetate, Glacial acetic acid or methyl ethyl diketone a kind of, sequestrant and ethanol, tetrabutyl titanate, the volume ratio of deionized water is 1～8:14～20:1～3:1～3, silane coupling agent with reactive epoxy group(ing) is γ-glycidyl ether oxygen propyl trimethoxy silicane, and solvent is toluene, ethanol, in methyl alcohol or the Virahol one or more;
C. prepare raspberry shape structure nano composite particles: with the described epoxy group modified titanium dioxide nano-particle of the described amido modified hollow silica Nano microsphere of steps A and step B take mass ratio as 1:0.8～2 ratio dispersion solvent in, stirring reaction is 8～12 hours between 20～50 ℃, obtains raspberry shape structure nano composite particles through washing drying;
D. prepare super hydrophobic surface: after above-mentioned raspberry shape structure nano composite particles and solvent, be coated to inorganic or the organic materials substrate on, and use long carbochain fluorine-containing material to modify, namely get super hydrophobic surface.
The present invention's employed solvent load in step B is 20～50 times that titanium dioxide nano-particle adds quality, and described solvent load is 100:3～5 with volume ratio with the silane coupling agent consumption of reactive epoxy group(ing).
The present invention's employed solvent in step C is one or more of toluene, ethanol, methyl alcohol or Virahol, and the consumption of solvent is 20～50 times of the described epoxy group modified titanium dioxide nano-particle total mass of the described amido modified hollow silica Nano microsphere of steps A and step B.
In addition, the present invention's employed solvent in step D is one or more of toluene, ethanol, methyl alcohol, and described long carbochain fluorine-containing material is 1H, 1H, 2H, 2H-perfluoro capryl Trimethoxy silane, perfluor dodecyltrichlorosilane or 1H, 1H, 2H, 2H-perfluor decyl mercaptan a kind of, described inorganic or organic materials is pottery, glass, semi-conductor, macromolecular material, and described hybrid mode is ultrasonic wave or mechanical stirring, described coating method is coated with for dripping, spraying or spin coating method a kind of.
The prepared super hydrophobic surface water contact angle of the present invention can reach 153o.Contain hollow structure in microtexture, and there is the titanium dioxide nano-particle of chemical bonding in the surface.Can be applicable to heavy metal ion adsorbed with separate, the Adsorption and decomposition of obnoxious flavour and the microcarrier aspect in the phase separation.
Embodiment
In order to understand better the present invention, describe by embodiment, but the present invention not merely is defined in this embodiment.
Embodiment 1
(1) the preparation mol ratio is the 3-TSL 8330 of 4:1 and mixture 1.2 grams of tetraethoxy, stirs it is mixed; Dropwise splash in the 8mL deionized water, mix solution with the speed of 200rpm, 20 ℃ of lower stirrings 4 hours, mixing solutions left standstill 10 hours, filtered and obtained precipitation, with washed with de-ionized water three times.
(2) 20mL dehydrated alcohol and 1mL methyl aceto acetate are mixed, again the 2mL tetrabutyl titanate is joined in the mixing solutions, stirred 1 hour.In 30 minutes, the 1mL deionized water is joined in the mixing solutions, stirred 10 hours with the speed of 600rpm, left standstill 24 hours, obtain yellow sol.With dehydrated alcohol centrifugal three times, 50 ℃ lower dry 12 hours, grind and make titanium dioxide nano-particle.Get 1.0 and restrain standby titanium dioxide nano-particle, be dispersed in 50mL3% γ-glycidyl ether oxygen propyl trimethoxy silicane ethanolic soln, 50 ℃ of lower backflows 8 hours, centrifugal three times of use dehydrated alcohol, 50 ℃ are lower dry 12 hours.
(3) get 0.5 gram step (1) preparation product and be dispersed in the 50mL dehydrated alcohol with 0.6 gram step (3) preparation product, 50 ℃ of lower backflows 12 hours are used dehydrated alcohol centrifugal three times, obtain product 50 ℃ of lower dryings 12 hours.
(4) get slide glass, at first use acetone to clean 10 minutes, then use dehydrated alcohol to clean 10 minutes, use at last distilled water to clean 10 minutes, above process all is to carry out seasoning under ul-trasonic irradiation.Step (3) products therefrom dripped be coated onto on the slide glass, after solvent evaporates, obtain the surface.The surface was immersed in the ethanolic soln of 3% perfluor dodecyltrichlorosilane 18 hours, and after surface drying, obtained surface, i.e. super hydrophobic surface.
Embodiment 2
(1) the preparation mol ratio is the 3-TSL 8330 of 3:1 and mixture 2.2 grams of tetraethoxy, stirs it is mixed; Dropwise splash in the 14mL deionized water, mix solution with the speed of 200rpm, 20 ℃ of lower stirrings 5 hours, mixing solutions left standstill 10 hours, filtered and obtained precipitation, with washed with de-ionized water three times.
(2) 14mL dehydrated alcohol and 7mL Glacial acetic acid are mixed, again the 1mL tetrabutyl titanate is joined in the mixing solutions, stirred 1 hour.In 30 minutes, the 3mL deionized water is joined in the mixing solutions, stirred 10 hours with the speed of 600rpm, left standstill 24 hours, obtain yellow sol.With dehydrated alcohol centrifugal three times, 50 ℃ lower dry 12 hours, grind and make titanium dioxide nano-particle.Get 1.0 and restrain standby TiO 2 particles, be dispersed in 50mL3% γ-glycidyl ether oxygen propyl trimethoxy silicane ethanolic soln, the speed with 200rpm under 20 ℃ stirred 12 hours, used dehydrated alcohol centrifugal three times, and 50 ℃ lower dry 12 hours.
(3) get 0.5 gram step (1) preparation product and be dispersed in the 50mL toluene with 0.55 gram step (3) preparation product, 50 ℃ of lower backflows 8 hours are used dehydrated alcohol centrifugal three times, obtain product 50 ℃ of lower dryings 12 hours.
(4) get slide glass, at first use acetone to clean 10 minutes, then use dehydrated alcohol to clean 10 minutes, use at last distilled water to clean 10 minutes, above process all is to carry out seasoning under ul-trasonic irradiation.Step (3) products therefrom is sprayed on the slide glass, after solvent evaporates, obtain the surface.3%1H is immersed on the surface, 1H, 2H in the ethanolic soln of 2H-perfluoro capryl Trimethoxy silane 18 hours, obtains surface, i.e. super hydrophobic surface after surface drying.
Embodiment 3
(1) the preparation mol ratio is the N-β (aminoethyl)-γ-aminopropyl methyl dimethoxysilane of 5:1 and mixture 1.5 grams of tetraethoxy, stirs it is mixed; Dropwise splash in the 10mL deionized water, mix solution with the speed of 200rpm, 30 ℃ of lower stirrings 4 hours, mixing solutions left standstill 10 hours, filtered and obtained precipitation, with washed with de-ionized water three times.
(2) 20mL dehydrated alcohol and 1mL methyl ethyl diketone are mixed, again the 3mL tetrabutyl titanate is joined in the mixing solutions, stirred 1 hour.In 30 minutes, the 1mL deionized water is joined in the mixing solutions, stirred 10 hours with the speed of 600rpm, left standstill 24 hours, obtain yellow sol.With dehydrated alcohol centrifugal three times, 50 ℃ lower dry 12 hours, grind and make titanium dioxide nano-particle.Get 1.0 and restrain standby titanium dioxide nano-particle, be dispersed in 50mL5% γ-glycidyl ether oxygen propyl trimethoxy silicane aqueous isopropanol, 50 ℃ of lower backflows 8 hours, centrifugal three times of use Virahol, 50 ℃ are lower dry 12 hours.
(3) get 0.5 gram step (1) preparation product and be dispersed in the 40mL Virahol with 0.5 gram step (3) preparation product, 50 ℃ of lower backflows 12 hours are used Virahol centrifugal three times, obtain product 50 ℃ of lower dryings 12 hours.
(4) get slide glass, at first use acetone to clean 10 minutes, then use dehydrated alcohol to clean 10 minutes, use at last distilled water to clean 10 minutes, above process all is to carry out seasoning under ul-trasonic irradiation.Step (3) products therefrom is spun on the slide glass, after solvent evaporates, obtains the surface.The surface was immersed in the ethanolic soln of 3% perfluor dodecyltrichlorosilane 18 hours, and after surface drying, obtained surface, i.e. super hydrophobic surface.
Claims (4)
1. the preparation method of a super hydrophobic surface is characterized in that the method mainly may further comprise the steps:
A. prepare amido modified hollow silica Nano microsphere: will be with the silane coupling agent of reactive amino and the mixture of tetraethoxy, be added drop-wise in the deionized water, stirring reaction is 2～8 hours between 20～40 ℃, obtain amido modified hollow silica Nano microsphere, wherein said silane coupling agent with reactive amino is APTES, the 3-TSL 8330, N-β (aminoethyl)-γ-aminopropyl methyl dimethoxysilane or N-β (aminoethyl)-γ-aminopropyl triethoxysilane a kind of, being 2～5:1 with the silane coupling agent consumption of reactive amino and the mol ratio of tetraethoxy consumption, is 1:4～8 with the silane coupling agent of reactive amino and the mixture of tetraethoxy and the mass ratio of deionized water;
B. prepare epoxy group modified titanium dioxide nano-particle: deionized water is added drop-wise to sequestrant, in the mixture of ethanol and tetrabutyl titanate, stirring reaction 8～12 hours, centrifugal drying, grind afterwards and make titanium dioxide nano-particle, with prepared titanium dioxide nano-particle with join respectively in the solvent with the silane coupling agent of reactive epoxy group(ing), stirring reaction is 8～12 hours between 30～60 ℃, grind afterwards and make epoxy group modified titanium dioxide nano-particle, wherein said sequestrant is methyl aceto acetate, Glacial acetic acid or methyl ethyl diketone a kind of, sequestrant and ethanol, tetrabutyl titanate, the volume ratio of deionized water is 1～8:14～20:1～3:1～3, silane coupling agent with reactive epoxy group(ing) is γ-glycidyl ether oxygen propyl trimethoxy silicane, and solvent is toluene, ethanol, in methyl alcohol or the Virahol one or more;
C. prepare raspberry shape structure nano composite particles: with the described epoxy group modified titanium dioxide nano-particle of the described amido modified hollow silica Nano microsphere of steps A and step B take mass ratio as 1:0.8～2 ratio is distributed in the solvent, stirring reaction is 8～12 hours between 20～50 ℃, obtains raspberry shape structure nano composite particles through washing drying;
D. prepare super hydrophobic surface: after above-mentioned raspberry shape structure nano composite particles and solvent, be coated to inorganic or the organic materials substrate on, and use long carbochain fluorine-containing material to modify, namely get super hydrophobic surface.
2. the preparation method of super hydrophobic surface according to claim 1, it is characterized in that: the solvent load described in the step B is 20～50 times that titanium dioxide nano-particle adds quality, and described solvent load is 100:3～5 with volume ratio with the silane coupling agent consumption of reactive epoxy group(ing).
3. the preparation method of super hydrophobic surface according to claim 1, it is characterized in that: the solvent described in the step C is one or more of toluene, ethanol, methyl alcohol or Virahol, and the consumption of solvent is 20～50 times of the described epoxy group modified titanium dioxide nano-particle total mass of the described amido modified hollow silica Nano microsphere of steps A and step B.
4. the preparation method of super hydrophobic surface according to claim 1, it is characterized in that: among the step D, described solvent is one or more of toluene, ethanol, methyl alcohol, described long carbochain fluorine-containing material is 1H, 1H, 2H, 2H-perfluoro capryl Trimethoxy silane, perfluor dodecyltrichlorosilane or 1H, 1H, 2H, 2H-perfluor decyl mercaptan a kind of, described inorganic or organic materials is pottery, glass, semi-conductor, macromolecular material, described hybrid mode is ultrasonic wave or mechanical stirring, described coating method is coated with for dripping, spraying or spin coating method a kind of.
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